Several wet digestion and dry ashing methods were compared for the voltammetric determination of arsenic (7440382), bismuth (7440699), cadmium (7440439), copper (7440508), lead (7439921), nickel (7440020), selenium (7782492), vanadium (7440622), and zinc (7440666) in biological and environmental materials. The methods tested included direct dry ashing, dry ashing with sulfuric-acid, nitric-acid, or magnesium-nitrate as ashing aids, wet digestion with nitric-acid only, wet digestion with a mixture of nitric-acid and sulfuric-acid, and wet digestion with a mixture of nitric-acid and potassium-persulfate. In general the wet digestion methods were faster than the dry ashing methods. However, larger amounts of reagents were needed for the wet methods, yielding higher blank contributions for some elements. The lower blank level was one of the main advantage of the dry ashing method, along with lower background current and an ability to handle considerably larger amounts of sample. It was necessary, however, to provide careful dissolution of the sample ash in a suitable reagent. Both decomposition methods allowed reliable voltammetric determination to be made of trace elements in biological and environmental materials with relative standard deviations between 1 and 3 percent. The amount of sample available, the nature of that sample, the sample matrix and the analysis time available each influenced the method chosen for the task.